# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yixia Ren' _publ_contact_author_email renyixia1@163.com _publ_author_name 'Lin-Pei Jin' data_101021a_0m _database_code_depnum_ccdc_archive 'CCDC 815043' #TrackingRef '4444_web_deposit_cif_file_0_YixiaRen_1298976645.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H12 N2 O7 Pb S' _chemical_formula_weight 631.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.0908(5) _cell_length_b 10.8703(8) _cell_length_c 26.4114(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.6080(10) _cell_angle_gamma 90.00 _cell_volume 2017.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2015 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 22.96 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 8.511 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2248 _exptl_absorpt_correction_T_max 0.6292 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9992 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3647 _reflns_number_gt 2816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3647 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6304(9) 0.2032(7) 0.4968(3) 0.0359(17) Uani 1 1 d . . . H1 H 0.6671 0.2632 0.5213 0.043 Uiso 1 1 calc R . . C2 C 0.7559(10) 0.1078(7) 0.4916(3) 0.047(2) Uani 1 1 d . . . H2 H 0.8737 0.1047 0.5117 0.056 Uiso 1 1 calc R . . C3 C 0.7036(10) 0.0193(8) 0.4564(3) 0.049(2) Uani 1 1 d . . . H3 H 0.7842 -0.0468 0.4530 0.059 Uiso 1 1 calc R . . C4 C 0.5285(10) 0.0273(7) 0.4253(3) 0.0399(18) Uani 1 1 d . . . C5 C 0.4631(12) -0.0630(8) 0.3876(4) 0.063(3) Uani 1 1 d . . . H5 H 0.5416 -0.1287 0.3819 0.076 Uiso 1 1 calc R . . C6 C 0.2917(13) -0.0542(8) 0.3607(3) 0.064(3) Uani 1 1 d . . . H6 H 0.2539 -0.1144 0.3364 0.077 Uiso 1 1 calc R . . C7 C 0.1641(11) 0.0430(7) 0.3672(3) 0.045(2) Uani 1 1 d . . . C8 C -0.0198(11) 0.0542(8) 0.3406(3) 0.054(2) Uani 1 1 d . . . H8 H -0.0644 -0.0042 0.3162 0.065 Uiso 1 1 calc R . . C9 C -0.1319(12) 0.1486(8) 0.3503(3) 0.055(2) Uani 1 1 d . . . H9 H -0.2546 0.1550 0.3330 0.067 Uiso 1 1 calc R . . C10 C -0.0636(10) 0.2362(7) 0.3860(3) 0.0405(19) Uani 1 1 d . . . H10 H -0.1415 0.3023 0.3917 0.049 Uiso 1 1 calc R . . C11 C 0.4081(9) 0.1254(6) 0.4333(2) 0.0280(16) Uani 1 1 d . . . C12 C 0.2215(9) 0.1340(6) 0.4044(2) 0.0313(17) Uani 1 1 d . . . C13 C 0.5110(8) 0.4742(6) 0.5968(2) 0.0244(15) Uani 1 1 d . . . C14 C 0.4453(8) 0.4003(6) 0.6397(2) 0.0250(14) Uani 1 1 d . . . C15 C 0.5792(9) 0.3814(6) 0.6822(2) 0.0339(17) Uani 1 1 d . . . H15 H 0.7005 0.4145 0.6830 0.041 Uiso 1 1 calc R . . C16 C 0.5346(9) 0.3141(7) 0.7231(2) 0.0380(18) Uani 1 1 d . . . H16 H 0.6283 0.2990 0.7505 0.046 Uiso 1 1 calc R . . C17 C 0.3555(9) 0.2690(6) 0.7243(2) 0.0337(17) Uani 1 1 d . . . C18 C 0.2992(11) 0.1971(7) 0.7677(3) 0.0399(18) Uani 1 1 d . . . C19 C 0.2169(9) 0.2878(6) 0.6819(2) 0.0305(16) Uani 1 1 d . . . H19 H 0.0943 0.2578 0.6821 0.037 Uiso 1 1 calc R . . C20 C 0.2624(8) 0.3511(6) 0.6396(2) 0.0241(15) Uani 1 1 d . . . N1 N 0.4619(7) 0.2140(5) 0.46932(19) 0.0294(13) Uani 1 1 d . . . N2 N 0.1085(7) 0.2298(5) 0.41262(19) 0.0297(13) Uani 1 1 d . . . O1 O 0.4939(6) 0.4305(4) 0.55282(15) 0.0330(12) Uani 1 1 d . . . O2 O 0.5936(7) 0.5737(4) 0.60895(15) 0.0341(11) Uani 1 1 d . . . O3 O 0.4329(7) 0.2011(5) 0.80825(17) 0.0492(14) Uani 1 1 d . . . H3A H 0.4151 0.1454 0.8280 0.074 Uiso 1 1 calc R . . O4 O 0.1539(8) 0.1399(6) 0.76700(19) 0.0671(18) Uani 1 1 d . . . O5 O -0.0971(6) 0.3402(5) 0.60521(17) 0.0505(15) Uani 1 1 d . . . O6 O 0.1260(6) 0.2754(4) 0.54856(16) 0.0340(11) Uani 1 1 d . . . O7 O 0.0945(6) 0.4904(4) 0.56714(16) 0.0387(12) Uani 1 1 d . . . Pb1 Pb 0.24935(3) 0.39768(2) 0.472234(9) 0.02365(9) Uani 1 1 d . . . S1 S 0.0802(2) 0.36540(16) 0.58644(6) 0.0295(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(4) 0.033(4) 0.040(4) -0.001(3) -0.013(3) 0.004(3) C2 0.043(4) 0.044(5) 0.050(5) 0.003(4) -0.004(4) 0.013(4) C3 0.038(4) 0.039(5) 0.074(6) 0.005(4) 0.021(4) 0.014(4) C4 0.039(4) 0.029(5) 0.054(5) -0.008(4) 0.012(4) 0.003(3) C5 0.058(6) 0.042(6) 0.094(8) -0.022(5) 0.025(5) 0.004(4) C6 0.074(6) 0.052(6) 0.068(6) -0.045(5) 0.014(5) -0.011(5) C7 0.060(5) 0.038(5) 0.038(5) -0.015(4) 0.005(4) -0.009(4) C8 0.060(5) 0.055(6) 0.043(5) -0.016(4) -0.012(4) -0.014(5) C9 0.055(5) 0.056(6) 0.047(5) -0.005(4) -0.025(4) -0.005(4) C10 0.040(4) 0.036(5) 0.040(5) -0.002(3) -0.012(4) 0.003(3) C11 0.030(3) 0.026(4) 0.030(4) -0.001(3) 0.008(3) -0.006(3) C12 0.036(4) 0.026(4) 0.030(4) -0.005(3) -0.002(3) -0.005(3) C13 0.027(3) 0.024(4) 0.021(4) -0.001(3) 0.001(3) 0.003(3) C14 0.032(3) 0.019(3) 0.022(3) -0.003(3) -0.002(3) 0.002(3) C15 0.034(4) 0.042(5) 0.024(4) 0.004(3) -0.004(3) -0.008(3) C16 0.037(4) 0.057(5) 0.018(4) 0.003(3) -0.007(3) 0.000(4) C17 0.042(4) 0.038(5) 0.020(4) 0.005(3) 0.000(3) -0.005(3) C18 0.049(5) 0.044(5) 0.026(4) 0.009(3) -0.001(4) -0.008(4) C19 0.028(4) 0.036(5) 0.026(4) -0.001(3) -0.002(3) -0.008(3) C20 0.027(3) 0.030(4) 0.015(3) 0.000(3) 0.000(3) 0.009(3) N1 0.030(3) 0.024(3) 0.033(3) -0.002(3) 0.003(3) 0.000(3) N2 0.037(3) 0.024(3) 0.027(3) -0.004(2) -0.002(3) 0.001(3) O1 0.035(3) 0.046(3) 0.017(2) -0.008(2) -0.001(2) -0.007(2) O2 0.055(3) 0.027(3) 0.022(3) -0.004(2) 0.011(2) -0.007(2) O3 0.064(3) 0.056(4) 0.024(3) 0.019(2) -0.006(3) -0.016(3) O4 0.069(4) 0.087(5) 0.042(4) 0.027(3) -0.002(3) -0.030(3) O5 0.022(2) 0.094(5) 0.036(3) 0.005(3) 0.006(2) 0.003(3) O6 0.041(3) 0.028(3) 0.031(3) 0.000(2) -0.002(2) 0.002(2) O7 0.048(3) 0.033(3) 0.032(3) 0.004(2) -0.004(2) 0.017(2) Pb1 0.02656(13) 0.02324(14) 0.02062(14) -0.00139(11) 0.00111(9) 0.00254(12) S1 0.0247(8) 0.0377(12) 0.0249(9) -0.0010(7) -0.0015(7) 0.0069(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.319(7) . ? C1 C2 1.385(9) . ? C1 H1 0.9300 . ? C2 C3 1.354(10) . ? C2 H2 0.9300 . ? C3 C4 1.398(9) . ? C3 H3 0.9300 . ? C4 C11 1.399(9) . ? C4 C5 1.430(10) . ? C5 C6 1.328(11) . ? C5 H5 0.9300 . ? C6 C7 1.417(11) . ? C6 H6 0.9300 . ? C7 C8 1.402(10) . ? C7 C12 1.415(9) . ? C8 C9 1.343(11) . ? C8 H8 0.9300 . ? C9 C10 1.383(10) . ? C9 H9 0.9300 . ? C10 N2 1.327(7) . ? C10 H10 0.9300 . ? C11 N1 1.373(8) . ? C11 C12 1.440(8) . ? C12 N2 1.349(8) . ? C13 O1 1.246(7) . ? C13 O2 1.252(7) . ? C13 C14 1.511(8) . ? C14 C15 1.386(8) . ? C14 C20 1.403(8) . ? C15 C16 1.376(9) . ? C15 H15 0.9300 . ? C16 C17 1.365(9) . ? C16 H16 0.9300 . ? C17 C19 1.404(8) . ? C17 C18 1.486(9) . ? C18 O4 1.201(8) . ? C18 O3 1.334(7) . ? C19 C20 1.385(8) . ? C19 H19 0.9300 . ? C20 S1 1.784(6) . ? N1 Pb1 2.509(5) . ? N2 Pb1 2.528(5) . ? O1 Pb1 2.586(4) . ? O1 Pb1 2.750(4) 3_666 ? O2 Pb1 2.563(4) 3_666 ? O3 H3A 0.8200 . ? O5 S1 1.438(4) . ? O6 S1 1.466(4) . ? O6 Pb1 2.658(4) . ? O7 S1 1.459(5) . ? Pb1 O2 2.563(4) 3_666 ? Pb1 O1 2.750(4) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.9(7) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 118.6(7) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 120.0(7) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C11 118.1(7) . . ? C3 C4 C5 123.2(7) . . ? C11 C4 C5 118.7(7) . . ? C6 C5 C4 120.8(8) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 122.9(7) . . ? C5 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C8 C7 C12 116.8(7) . . ? C8 C7 C6 124.8(7) . . ? C12 C7 C6 118.4(7) . . ? C9 C8 C7 120.4(7) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.6(7) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 122.7(7) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? N1 C11 C4 121.3(6) . . ? N1 C11 C12 118.2(6) . . ? C4 C11 C12 120.4(6) . . ? N2 C12 C7 121.9(6) . . ? N2 C12 C11 119.3(6) . . ? C7 C12 C11 118.8(6) . . ? O1 C13 O2 123.6(6) . . ? O1 C13 C14 119.6(6) . . ? O2 C13 C14 116.6(5) . . ? C15 C14 C20 118.6(6) . . ? C15 C14 C13 116.1(5) . . ? C20 C14 C13 125.3(5) . . ? C16 C15 C14 120.7(6) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 121.3(6) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C19 119.0(6) . . ? C16 C17 C18 123.5(6) . . ? C19 C17 C18 117.5(6) . . ? O4 C18 O3 123.1(6) . . ? O4 C18 C17 125.3(6) . . ? O3 C18 C17 111.6(6) . . ? C20 C19 C17 120.2(6) . . ? C20 C19 H19 119.9 . . ? C17 C19 H19 119.9 . . ? C19 C20 C14 120.1(5) . . ? C19 C20 S1 117.1(5) . . ? C14 C20 S1 122.8(5) . . ? C1 N1 C11 117.9(6) . . ? C1 N1 Pb1 123.9(4) . . ? C11 N1 Pb1 117.8(4) . . ? C10 N2 C12 118.7(6) . . ? C10 N2 Pb1 123.5(4) . . ? C12 N2 Pb1 117.6(4) . . ? C13 O1 Pb1 142.3(4) . . ? C13 O1 Pb1 88.8(4) . 3_666 ? Pb1 O1 Pb1 106.79(15) . 3_666 ? C13 O2 Pb1 97.5(4) . 3_666 ? C18 O3 H3A 109.5 . . ? S1 O6 Pb1 108.0(2) . . ? N1 Pb1 N2 66.15(16) . . ? N1 Pb1 O2 75.03(15) . 3_666 ? N2 Pb1 O2 75.30(15) . 3_666 ? N1 Pb1 O1 78.15(15) . . ? N2 Pb1 O1 141.13(16) . . ? O2 Pb1 O1 110.70(14) 3_666 . ? N1 Pb1 O6 83.37(15) . . ? N2 Pb1 O6 88.21(15) . . ? O2 Pb1 O6 156.72(14) 3_666 . ? O1 Pb1 O6 72.35(13) . . ? N1 Pb1 O1 96.54(15) . 3_666 ? N2 Pb1 O1 124.07(15) . 3_666 ? O2 Pb1 O1 48.80(13) 3_666 3_666 ? O1 Pb1 O1 73.21(15) . 3_666 ? O6 Pb1 O1 144.80(12) . 3_666 ? O5 S1 O7 113.7(3) . . ? O5 S1 O6 113.0(3) . . ? O7 S1 O6 110.5(3) . . ? O5 S1 C20 106.7(3) . . ? O7 S1 C20 106.2(3) . . ? O6 S1 C20 106.0(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.645 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.148 # Attachment '4445_web_deposit_cif_file_1_YixiaRen_1298976645.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 815044' #TrackingRef '4445_web_deposit_cif_file_1_YixiaRen_1298976645.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 N2 O9 Pb S' _chemical_formula_weight 643.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3160(14) _cell_length_b 10.8418(14) _cell_length_c 12.355(3) _cell_angle_alpha 80.397(3) _cell_angle_beta 87.938(2) _cell_angle_gamma 83.928(2) _cell_volume 960.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1420 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 8.948 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2958 _exptl_absorpt_correction_T_max 0.4131 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4902 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3446 _reflns_number_gt 3012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+2.9706P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3446 _refine_ls_number_parameters 288 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.69934(4) 0.72859(3) 0.20974(2) 0.02404(11) Uani 1 1 d . . . S1 S 0.1970(2) 0.84478(19) 0.20228(15) 0.0243(4) Uani 1 1 d . . . O1 O 0.4890(7) 0.5808(5) 0.3080(5) 0.0405(15) Uani 1 1 d . . . O2 O 0.2328(7) 0.5285(5) 0.3983(5) 0.0368(14) Uani 1 1 d . . . O3 O 0.1087(8) 0.9690(5) 0.1630(4) 0.0400(15) Uani 1 1 d . . . O4 O 0.3712(7) 0.8206(7) 0.1458(4) 0.0458(17) Uani 1 1 d . . . O5 O 0.0794(7) 0.7452(5) 0.2017(5) 0.0357(14) Uani 1 1 d . . . O6 O 0.2826(9) 1.0682(6) 0.6413(5) 0.0493(17) Uani 1 1 d . . . O7 O 0.1683(9) 1.1664(6) 0.4802(5) 0.0406(15) Uani 1 1 d . . . H7 H 0.1389 1.2232 0.5157 0.061 Uiso 1 1 calc R . . O8 O 0.7593(9) 0.9617(7) 0.0835(6) 0.064(2) Uani 1 1 d D . . H8A H 0.8702(15) 0.9613(7) 0.0961(6) 0.096 Uiso 1 1 d RD . . H8B H 0.7262(10) 1.0156(9) 0.0266(9) 0.096 Uiso 1 1 d RD . . O9 O 0.8749(7) 0.6324(5) 0.4224(5) 0.0335(13) Uani 1 1 d D . . H9A H 0.985(5) 0.603(7) 0.407(7) 0.050 Uiso 1 1 d D . . H9B H 0.830(9) 0.578(6) 0.471(6) 0.050 Uiso 1 1 d D . . N1 N 0.8109(8) 0.5102(6) 0.1684(5) 0.0275(15) Uani 1 1 d . . . N2 N 0.6615(8) 0.6968(7) 0.0138(5) 0.0285(15) Uani 1 1 d . . . C1 C 0.8787(12) 0.4205(8) 0.2470(7) 0.038(2) Uani 1 1 d . . . H1 H 0.8947 0.4409 0.3160 0.046 Uiso 1 1 calc R . . C2 C 0.9263(12) 0.2994(8) 0.2315(8) 0.043(2) Uani 1 1 d . . . H2 H 0.9733 0.2391 0.2889 0.052 Uiso 1 1 calc R . . C3 C 0.9040(11) 0.2677(8) 0.1302(8) 0.041(2) Uani 1 1 d . . . H3 H 0.9370 0.1860 0.1179 0.050 Uiso 1 1 calc R . . C4 C 0.8316(12) 0.3591(9) 0.0467(7) 0.040(2) Uani 1 1 d . . . H4 H 0.8135 0.3396 -0.0224 0.048 Uiso 1 1 calc R . . C5 C 0.7865(10) 0.4807(8) 0.0680(6) 0.0293(18) Uani 1 1 d . . . C6 C 0.7080(10) 0.5824(8) -0.0167(6) 0.0265(17) Uani 1 1 d . . . C7 C 0.6847(11) 0.5685(9) -0.1256(7) 0.037(2) Uani 1 1 d . . . H7A H 0.7146 0.4904 -0.1470 0.044 Uiso 1 1 calc R . . C8 C 0.6176(12) 0.6696(10) -0.2017(7) 0.044(2) Uani 1 1 d . . . H8 H 0.6042 0.6601 -0.2743 0.053 Uiso 1 1 calc R . . C9 C 0.5705(11) 0.7845(9) -0.1699(7) 0.038(2) Uani 1 1 d . . . H9 H 0.5242 0.8537 -0.2198 0.046 Uiso 1 1 calc R . . C10 C 0.5945(11) 0.7939(8) -0.0600(6) 0.0319(19) Uani 1 1 d . . . H10 H 0.5624 0.8710 -0.0373 0.038 Uiso 1 1 calc R . . C11 C 0.3484(9) 0.6046(7) 0.3663(6) 0.0230(16) Uani 1 1 d . . . C12 C 0.3231(10) 0.7280(8) 0.4073(6) 0.0285(18) Uani 1 1 d . . . C13 C 0.2522(9) 0.8419(7) 0.3417(6) 0.0232(16) Uani 1 1 d . . . C14 C 0.2247(9) 0.9528(7) 0.3855(6) 0.0241(17) Uani 1 1 d . . . H14 H 0.1761 1.0270 0.3427 0.029 Uiso 1 1 calc R . . C15 C 0.2708(10) 0.9515(8) 0.4946(6) 0.0261(17) Uani 1 1 d . . . C16 C 0.2418(10) 1.0651(8) 0.5468(7) 0.0300(19) Uani 1 1 d . . . C17 C 0.3401(11) 0.8396(8) 0.5577(7) 0.034(2) Uani 1 1 d . . . H17 H 0.3688 0.8393 0.6305 0.041 Uiso 1 1 calc R . . C18 C 0.3677(11) 0.7295(8) 0.5163(6) 0.034(2) Uani 1 1 d . . . H18 H 0.4158 0.6560 0.5604 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02360(16) 0.02444(17) 0.02505(16) -0.00725(12) 0.00116(10) -0.00238(12) S1 0.0220(9) 0.0288(11) 0.0218(9) -0.0046(8) -0.0014(7) 0.0005(8) O1 0.034(3) 0.030(3) 0.058(4) -0.011(3) 0.015(3) -0.007(3) O2 0.033(3) 0.029(3) 0.048(4) -0.006(3) 0.013(3) -0.010(3) O3 0.053(4) 0.033(3) 0.033(3) -0.001(3) -0.019(3) -0.002(3) O4 0.028(3) 0.080(5) 0.027(3) -0.012(3) 0.003(2) 0.006(3) O5 0.033(3) 0.038(3) 0.040(3) -0.013(3) -0.007(2) -0.008(3) O6 0.066(4) 0.051(4) 0.032(3) -0.014(3) -0.009(3) 0.003(4) O7 0.057(4) 0.027(3) 0.039(3) -0.013(3) -0.006(3) 0.008(3) O8 0.050(4) 0.060(5) 0.075(5) 0.018(4) -0.028(4) -0.013(4) O9 0.034(3) 0.032(3) 0.035(3) -0.004(3) 0.004(2) -0.004(3) N1 0.027(3) 0.025(4) 0.030(4) -0.008(3) 0.004(3) 0.001(3) N2 0.032(3) 0.040(4) 0.013(3) -0.004(3) -0.001(3) 0.004(3) C1 0.044(5) 0.037(5) 0.031(5) -0.002(4) -0.001(4) -0.002(4) C2 0.049(6) 0.023(5) 0.051(6) 0.008(4) 0.005(4) 0.002(4) C3 0.028(4) 0.028(5) 0.067(7) -0.012(5) 0.012(4) 0.001(4) C4 0.042(5) 0.040(5) 0.043(5) -0.018(4) -0.005(4) -0.005(4) C5 0.024(4) 0.035(5) 0.032(4) -0.013(4) 0.012(3) -0.009(4) C6 0.018(4) 0.031(5) 0.034(4) -0.013(4) 0.007(3) -0.010(3) C7 0.044(5) 0.037(5) 0.032(5) -0.017(4) -0.003(4) 0.005(4) C8 0.045(5) 0.065(7) 0.025(4) -0.009(5) -0.009(4) -0.008(5) C9 0.039(5) 0.047(6) 0.029(4) -0.007(4) -0.007(4) -0.002(4) C10 0.040(5) 0.034(5) 0.022(4) -0.009(4) 0.006(3) -0.003(4) C11 0.020(4) 0.022(4) 0.026(4) -0.001(3) 0.001(3) -0.002(3) C12 0.025(4) 0.032(5) 0.027(4) -0.007(4) 0.005(3) 0.003(4) C13 0.020(4) 0.027(4) 0.022(4) -0.002(3) 0.000(3) -0.004(3) C14 0.021(4) 0.023(4) 0.029(4) -0.010(3) 0.002(3) 0.003(3) C15 0.021(4) 0.032(5) 0.026(4) -0.012(4) 0.002(3) 0.001(3) C16 0.022(4) 0.037(5) 0.034(5) -0.015(4) 0.003(3) -0.003(4) C17 0.040(5) 0.027(5) 0.031(4) 0.002(4) -0.004(4) 0.005(4) C18 0.040(5) 0.041(5) 0.019(4) -0.007(4) -0.006(3) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O1 2.479(6) . ? Pb1 N2 2.530(6) . ? Pb1 N1 2.549(6) . ? Pb1 O4 2.598(5) . ? S1 O3 1.445(6) . ? S1 O5 1.451(6) . ? S1 O4 1.451(5) . ? S1 C13 1.777(7) . ? O1 C11 1.263(8) . ? O2 C11 1.252(9) . ? O6 C16 1.222(9) . ? O7 C16 1.333(10) . ? O7 H7 0.8200 . ? O8 H8A 0.8315 . ? O8 H8B 0.8598 . ? O9 H9A 0.86(2) . ? O9 H9B 0.85(2) . ? N1 C1 1.324(10) . ? N1 C5 1.354(10) . ? N2 C10 1.335(10) . ? N2 C6 1.362(10) . ? C1 C2 1.365(12) . ? C1 H1 0.9300 . ? C2 C3 1.371(13) . ? C2 H2 0.9300 . ? C3 C4 1.383(12) . ? C3 H3 0.9300 . ? C4 C5 1.391(12) . ? C4 H4 0.9300 . ? C5 C6 1.472(11) . ? C6 C7 1.397(11) . ? C7 C8 1.379(12) . ? C7 H7A 0.9300 . ? C8 C9 1.374(13) . ? C8 H8 0.9300 . ? C9 C10 1.397(11) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.499(11) . ? C12 C18 1.400(10) . ? C12 C13 1.419(11) . ? C13 C14 1.392(11) . ? C14 C15 1.398(10) . ? C14 H14 0.9300 . ? C15 C17 1.386(11) . ? C15 C16 1.476(11) . ? C17 C18 1.369(12) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 N2 100.6(2) . . ? O1 Pb1 N1 72.64(19) . . ? N2 Pb1 N1 64.4(2) . . ? O1 Pb1 O4 74.4(2) . . ? N2 Pb1 O4 70.89(18) . . ? N1 Pb1 O4 116.8(2) . . ? O3 S1 O5 113.7(3) . . ? O3 S1 O4 111.8(4) . . ? O5 S1 O4 111.8(4) . . ? O3 S1 C13 106.7(3) . . ? O5 S1 C13 106.5(3) . . ? O4 S1 C13 105.7(3) . . ? C11 O1 Pb1 128.5(5) . . ? S1 O4 Pb1 134.1(3) . . ? C16 O7 H7 109.5 . . ? H8A O8 H8B 111.7 . . ? H9A O9 H9B 108(3) . . ? C1 N1 C5 118.7(7) . . ? C1 N1 Pb1 120.7(5) . . ? C5 N1 Pb1 120.4(5) . . ? C10 N2 C6 120.0(7) . . ? C10 N2 Pb1 119.2(5) . . ? C6 N2 Pb1 120.8(5) . . ? N1 C1 C2 123.0(9) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.2(8) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 119.1(8) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 118.7(8) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 121.3(8) . . ? N1 C5 C6 117.1(7) . . ? C4 C5 C6 121.6(8) . . ? N2 C6 C7 119.2(7) . . ? N2 C6 C5 117.0(7) . . ? C7 C6 C5 123.7(7) . . ? C8 C7 C6 120.5(8) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C9 C8 C7 119.9(8) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 117.7(8) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? N2 C10 C9 122.8(8) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? O2 C11 O1 124.2(7) . . ? O2 C11 C12 116.9(6) . . ? O1 C11 C12 118.7(7) . . ? C18 C12 C13 118.9(7) . . ? C18 C12 C11 118.1(7) . . ? C13 C12 C11 123.0(7) . . ? C14 C13 C12 120.5(7) . . ? C14 C13 S1 119.1(6) . . ? C12 C13 S1 120.4(6) . . ? C13 C14 C15 119.4(7) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C17 C15 C14 119.5(7) . . ? C17 C15 C16 118.3(7) . . ? C14 C15 C16 122.2(7) . . ? O6 C16 O7 122.5(8) . . ? O6 C16 C15 124.1(8) . . ? O7 C16 C15 113.5(7) . . ? C18 C17 C15 122.0(8) . . ? C18 C17 H17 119.0 . . ? C15 C17 H17 119.0 . . ? C17 C18 C12 119.7(8) . . ? C17 C18 H18 120.2 . . ? C12 C18 H18 120.2 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.859 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.183 # Attachment '4446_web_deposit_cif_file_2_YixiaRen_1298976645.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 815045' #TrackingRef '4446_web_deposit_cif_file_2_YixiaRen_1298976645.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 N2 O8 Pb S' _chemical_formula_weight 625.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.2816(15) _cell_length_b 6.9457(6) _cell_length_c 14.1263(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.807(2) _cell_angle_gamma 90.00 _cell_volume 1858.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1273 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 20.52 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 9.244 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2470 _exptl_absorpt_correction_T_max 0.8367 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10673 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.56 _reflns_number_total 4237 _reflns_number_gt 3011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0045P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4237 _refine_ls_number_parameters 277 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4102(4) 0.8050(10) 0.2240(5) 0.0192(16) Uani 1 1 d . . . C2 C 0.3401(4) 0.7864(9) 0.2585(5) 0.0180(15) Uani 1 1 d . . . C3 C 0.2805(4) 0.7476(10) 0.1880(6) 0.0270(18) Uani 1 1 d . . . H3 H 0.2848 0.7312 0.1240 0.032 Uiso 1 1 calc R . . C4 C 0.2151(4) 0.7340(11) 0.2145(6) 0.033(2) Uani 1 1 d . . . H4 H 0.1754 0.7060 0.1681 0.040 Uiso 1 1 calc R . . C5 C 0.2080(4) 0.7616(11) 0.3100(6) 0.0287(19) Uani 1 1 d . . . C6 C 0.1363(4) 0.7527(12) 0.3358(7) 0.037(2) Uani 1 1 d . . . C7 C 0.2676(4) 0.8022(9) 0.3792(6) 0.0237(18) Uani 1 1 d . . . H7 H 0.2633 0.8217 0.4429 0.028 Uiso 1 1 calc R . . C8 C 0.3340(4) 0.8137(9) 0.3532(6) 0.0204(16) Uani 1 1 d . . . C9 C 0.2616(4) 0.2816(11) 0.3207(6) 0.032(2) Uani 1 1 d . . . H9 H 0.2658 0.2569 0.2573 0.039 Uiso 1 1 calc R . . C10 C 0.1961(4) 0.2550(11) 0.3457(6) 0.032(2) Uani 1 1 d . . . H10 H 0.1576 0.2140 0.3003 0.038 Uiso 1 1 calc R . . C11 C 0.1895(4) 0.2913(10) 0.4407(6) 0.0251(17) Uani 1 1 d . . . C12 C 0.2476(4) 0.3539(11) 0.5035(6) 0.0325(19) Uani 1 1 d . . . H12 H 0.2454 0.3789 0.5676 0.039 Uiso 1 1 calc R . . C13 C 0.3101(4) 0.3794(11) 0.4698(6) 0.0311(18) Uani 1 1 d . . . H13 H 0.3487 0.4279 0.5127 0.037 Uiso 1 1 calc R . . C14 C 0.1201(4) 0.2699(11) 0.4716(7) 0.032(2) Uani 1 1 d . . . C15 C 0.0567(4) 0.3017(12) 0.4081(7) 0.041(2) Uani 1 1 d . . . H15 H 0.0567 0.3376 0.3446 0.049 Uiso 1 1 calc R . . C16 C -0.0058(4) 0.2795(12) 0.4400(7) 0.038(2) Uani 1 1 d . . . H16 H -0.0477 0.2976 0.3959 0.045 Uiso 1 1 calc R . . C17 C 0.0503(5) 0.2018(13) 0.5911(7) 0.046(2) Uani 1 1 d . . . H17 H 0.0487 0.1674 0.6543 0.056 Uiso 1 1 calc R . . C18 C 0.1162(4) 0.2177(13) 0.5647(7) 0.041(2) Uani 1 1 d . . . H18 H 0.1572 0.1932 0.6094 0.049 Uiso 1 1 calc R . . N1 N 0.3188(3) 0.3403(8) 0.3817(5) 0.0280(16) Uani 1 1 d . . . N2 N -0.0103(4) 0.2334(11) 0.5305(6) 0.044(2) Uani 1 1 d . . . O1 O 0.4578(3) 0.6840(6) 0.2482(4) 0.0263(13) Uani 1 1 d . . . O2 O 0.4148(2) 0.9447(6) 0.1673(4) 0.0233(12) Uani 1 1 d . . . O3 O 0.0843(3) 0.7162(12) 0.2771(5) 0.070(2) Uani 1 1 d . . . O4 O 0.1363(3) 0.7863(8) 0.4259(5) 0.0480(17) Uani 1 1 d . . . H4A H 0.0958 0.7798 0.4358 0.072 Uiso 1 1 calc R . . O5 O 0.3812(3) 0.9451(7) 0.5247(4) 0.0291(12) Uani 1 1 d . . . O6 O 0.4481(3) 0.6915(6) 0.4662(4) 0.0261(12) Uani 1 1 d . . . O7 O 0.4474(3) 1.0112(6) 0.3977(4) 0.0263(12) Uani 1 1 d . . . O8 O 0.3841(3) 0.3173(7) 0.1904(4) 0.0309(13) Uani 1 1 d D . . H8A H 0.391(4) 0.382(8) 0.141(4) 0.046 Uiso 1 1 d D . . H8B H 0.383(4) 0.198(3) 0.176(5) 0.046 Uiso 1 1 d D . . Pb1 Pb 0.458052(13) 0.37665(4) 0.35276(2) 0.01961(9) Uani 1 1 d . . . S1 S 0.40876(9) 0.8718(2) 0.44380(13) 0.0190(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(4) 0.027(4) 0.016(4) -0.011(3) 0.007(3) -0.001(3) C2 0.023(4) 0.012(3) 0.018(4) 0.003(3) 0.002(3) 0.004(3) C3 0.017(4) 0.044(4) 0.019(5) -0.007(4) 0.000(3) -0.002(3) C4 0.021(4) 0.043(5) 0.034(6) 0.008(4) -0.001(4) -0.002(4) C5 0.019(4) 0.034(4) 0.035(6) 0.002(4) 0.010(4) -0.002(3) C6 0.032(5) 0.052(5) 0.030(6) 0.006(4) 0.009(4) 0.005(4) C7 0.022(4) 0.023(4) 0.030(5) 0.001(3) 0.014(3) 0.007(3) C8 0.025(4) 0.017(3) 0.022(5) 0.002(3) 0.011(3) 0.001(3) C9 0.033(5) 0.036(4) 0.032(6) -0.008(4) 0.015(4) -0.008(4) C10 0.015(4) 0.048(5) 0.035(6) 0.000(4) 0.009(4) -0.003(4) C11 0.026(4) 0.024(4) 0.027(5) 0.005(3) 0.010(3) -0.001(3) C12 0.030(4) 0.041(5) 0.030(5) 0.001(4) 0.013(4) -0.005(4) C13 0.022(4) 0.046(4) 0.022(5) 0.010(4) -0.003(3) -0.005(4) C14 0.025(4) 0.032(4) 0.040(6) -0.012(4) 0.010(4) 0.001(4) C15 0.027(5) 0.064(6) 0.034(6) 0.003(5) 0.013(4) -0.009(4) C16 0.016(4) 0.064(6) 0.035(6) -0.007(5) 0.006(4) 0.000(4) C17 0.035(5) 0.082(7) 0.025(6) -0.007(5) 0.016(4) -0.012(5) C18 0.028(5) 0.067(6) 0.029(6) 0.007(5) 0.006(4) 0.000(4) N1 0.022(3) 0.033(4) 0.032(4) 0.001(3) 0.012(3) -0.001(3) N2 0.022(4) 0.067(5) 0.046(6) -0.002(4) 0.018(4) -0.005(4) O1 0.028(3) 0.024(3) 0.031(4) 0.004(2) 0.018(2) 0.003(2) O2 0.026(3) 0.023(2) 0.024(3) 0.009(2) 0.013(2) 0.004(2) O3 0.020(3) 0.152(7) 0.038(5) 0.000(5) 0.003(3) -0.014(4) O4 0.021(3) 0.078(4) 0.051(5) -0.007(4) 0.022(3) -0.006(3) O5 0.033(3) 0.039(3) 0.017(3) -0.008(2) 0.007(2) 0.003(2) O6 0.029(3) 0.022(3) 0.025(3) 0.003(2) 0.001(2) 0.004(2) O7 0.028(3) 0.025(3) 0.028(3) 0.006(2) 0.011(2) -0.005(2) O8 0.046(4) 0.022(3) 0.025(4) -0.002(2) 0.009(3) 0.002(3) Pb1 0.01791(14) 0.01970(13) 0.02276(16) 0.00030(14) 0.00773(10) -0.00058(13) S1 0.0196(9) 0.0199(8) 0.0177(10) -0.0002(8) 0.0041(7) 0.0001(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.245(8) . ? C1 O2 1.272(8) . ? C1 C2 1.525(9) . ? C2 C8 1.379(10) . ? C2 C3 1.398(10) . ? C3 C4 1.385(9) . ? C3 H3 0.9300 . ? C4 C5 1.394(11) . ? C4 H4 0.9300 . ? C5 C7 1.390(11) . ? C5 C6 1.495(10) . ? C6 O3 1.202(11) . ? C6 O4 1.294(10) . ? C7 C8 1.397(9) . ? C7 H7 0.9300 . ? C8 S1 1.785(8) . ? C9 N1 1.331(10) . ? C9 C10 1.386(9) . ? C9 H9 0.9300 . ? C10 C11 1.394(11) . ? C10 H10 0.9300 . ? C11 C12 1.364(11) . ? C11 C14 1.491(10) . ? C12 C13 1.389(9) . ? C12 H12 0.9300 . ? C13 N1 1.314(9) . ? C13 H13 0.9300 . ? C14 C18 1.379(11) . ? C14 C15 1.392(12) . ? C15 C16 1.374(10) . ? C15 H15 0.9300 . ? C16 N2 1.337(11) . ? C16 H16 0.9300 . ? C17 N2 1.331(11) . ? C17 C18 1.394(10) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? O1 Pb1 2.596(5) . ? O1 Pb1 2.706(4) 2_655 ? O2 Pb1 2.564(4) 2_655 ? O4 H4A 0.8200 . ? O5 S1 1.440(5) . ? O6 S1 1.468(5) . ? O6 Pb1 2.739(5) . ? O7 S1 1.449(5) . ? O7 Pb1 2.634(4) 1_565 ? O8 Pb1 2.497(6) . ? O8 H8A 0.85(2) . ? O8 H8B 0.85(2) . ? Pb1 O2 2.564(4) 2_645 ? Pb1 O7 2.634(4) 1_545 ? Pb1 O1 2.706(4) 2_645 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 123.5(6) . . ? O1 C1 C2 120.5(6) . . ? O2 C1 C2 115.9(6) . . ? C8 C2 C3 120.6(7) . . ? C8 C2 C1 122.7(7) . . ? C3 C2 C1 116.6(7) . . ? C4 C3 C2 119.3(8) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.8(8) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C7 C5 C4 119.3(7) . . ? C7 C5 C6 121.2(8) . . ? C4 C5 C6 119.5(8) . . ? O3 C6 O4 124.2(8) . . ? O3 C6 C5 122.1(9) . . ? O4 C6 C5 113.8(8) . . ? C5 C7 C8 120.3(7) . . ? C5 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C2 C8 C7 119.7(7) . . ? C2 C8 S1 121.5(5) . . ? C7 C8 S1 118.8(6) . . ? N1 C9 C10 124.1(8) . . ? N1 C9 H9 118.0 . . ? C10 C9 H9 118.0 . . ? C9 C10 C11 118.2(8) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C12 C11 C10 118.2(7) . . ? C12 C11 C14 120.9(8) . . ? C10 C11 C14 120.9(7) . . ? C11 C12 C13 118.5(8) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? N1 C13 C12 124.9(7) . . ? N1 C13 H13 117.6 . . ? C12 C13 H13 117.6 . . ? C18 C14 C15 117.3(7) . . ? C18 C14 C11 121.2(8) . . ? C15 C14 C11 121.5(8) . . ? C16 C15 C14 119.3(9) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? N2 C16 C15 123.9(8) . . ? N2 C16 H16 118.0 . . ? C15 C16 H16 118.0 . . ? N2 C17 C18 123.3(9) . . ? N2 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C14 C18 C17 119.4(8) . . ? C14 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C13 N1 C9 116.1(6) . . ? C17 N2 C16 116.7(7) . . ? C1 O1 Pb1 129.4(4) . . ? C1 O1 Pb1 90.3(4) . 2_655 ? Pb1 O1 Pb1 140.29(19) . 2_655 ? C1 O2 Pb1 96.4(4) . 2_655 ? C6 O4 H4A 109.5 . . ? S1 O6 Pb1 130.2(3) . . ? S1 O7 Pb1 145.3(3) . 1_565 ? Pb1 O8 H8A 121(5) . . ? Pb1 O8 H8B 111(5) . . ? H8A O8 H8B 109(3) . . ? O8 Pb1 O2 108.77(17) . 2_645 ? O8 Pb1 O1 70.92(16) . . ? O2 Pb1 O1 71.65(15) 2_645 . ? O8 Pb1 O7 90.32(16) . 1_545 ? O2 Pb1 O7 108.87(14) 2_645 1_545 ? O1 Pb1 O7 159.70(16) . 1_545 ? O8 Pb1 O1 74.32(17) . 2_645 ? O2 Pb1 O1 49.68(14) 2_645 2_645 ? O1 Pb1 O1 92.52(7) . 2_645 ? O7 Pb1 O1 74.44(14) 1_545 2_645 ? O8 Pb1 O6 125.35(15) . . ? O2 Pb1 O6 95.21(14) 2_645 . ? O1 Pb1 O6 71.55(15) . . ? O7 Pb1 O6 127.68(15) 1_545 . ? O1 Pb1 O6 144.87(14) 2_645 . ? O5 S1 O7 114.7(3) . . ? O5 S1 O6 112.5(3) . . ? O7 S1 O6 112.2(3) . . ? O5 S1 C8 106.2(3) . . ? O7 S1 C8 104.1(3) . . ? O6 S1 C8 106.1(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.958 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.210 # Attachment '4447_web_deposit_cif_file_3_YixiaRen_1298976645.cif' data_101018b_0m _database_code_depnum_ccdc_archive 'CCDC 815046' #TrackingRef '4447_web_deposit_cif_file_3_YixiaRen_1298976645.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 O8 Pb S' _chemical_formula_weight 469.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9149(14) _cell_length_b 7.2161(8) _cell_length_c 12.6352(14) _cell_angle_alpha 90.00 _cell_angle_beta 103.615(2) _cell_angle_gamma 90.00 _cell_volume 1055.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1291 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 26.58 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 16.210 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1584 _exptl_absorpt_correction_T_max 0.4979 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6151 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.61 _reflns_number_total 2425 _reflns_number_gt 1819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0043(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2425 _refine_ls_number_parameters 171 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6354(6) 0.2536(9) 0.9407(5) 0.0099(13) Uani 1 1 d . . . C2 C 0.7560(6) 0.2290(8) 0.9240(5) 0.0071(13) Uani 1 1 d . . . C3 C 0.8475(6) 0.3032(8) 1.0007(5) 0.0100(14) Uani 1 1 d U . . H3 H 0.8336 0.3736 1.0598 0.012 Uiso 1 1 calc R . . C4 C 0.9598(6) 0.2742(8) 0.9908(6) 0.0119(14) Uani 1 1 d . . . H4 H 1.0224 0.3225 1.0446 0.014 Uiso 1 1 calc R . . C5 C 0.9820(6) 0.1763(8) 0.9039(5) 0.0093(14) Uani 1 1 d . . . C6 C 1.1057(6) 0.1487(9) 0.8994(6) 0.0130(15) Uani 1 1 d . . . C7 C 0.8916(6) 0.1054(9) 0.8249(6) 0.0136(15) Uani 1 1 d . . . H7 H 0.9068 0.0409 0.7642 0.016 Uiso 1 1 calc R . . C8 C 0.7785(6) 0.1285(8) 0.8342(5) 0.0090(14) Uani 1 1 d U . . O1 O 0.5903(4) 0.1134(6) 0.9750(4) 0.0145(11) Uani 1 1 d . . . O2 O 0.5877(4) 0.4071(6) 0.9252(4) 0.0135(11) Uani 1 1 d . . . O3 O 1.1848(4) 0.1853(7) 0.9766(4) 0.0177(11) Uani 1 1 d . . . O4 O 1.1186(4) 0.0817(7) 0.8059(4) 0.0220(12) Uani 1 1 d . . . H4A H 1.1887 0.0847 0.8046 0.033 Uiso 1 1 calc R . . O5 O 0.6165(4) -0.1178(6) 0.7935(4) 0.0136(11) Uani 1 1 d . . . O6 O 0.7134(4) -0.0465(6) 0.6511(3) 0.0102(10) Uani 1 1 d U . . O7 O 0.5827(4) 0.1810(6) 0.7014(4) 0.0158(11) Uani 1 1 d . . . O8 O 0.6569(4) -0.0628(6) 1.1880(4) 0.0130(10) Uani 1 1 d D . . H8A H 0.641(6) -0.134(6) 1.235(5) 0.020 Uiso 1 1 d D . . H8B H 0.625(6) 0.042(5) 1.189(5) 0.020 Uiso 1 1 d D . . Pb1 Pb 0.59321(2) -0.24036(3) 0.986690(19) 0.00932(11) Uani 1 1 d . . . S1 S 0.66362(15) 0.0294(2) 0.73705(13) 0.0093(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.008(3) 0.012(3) 0.012(3) 0.000(3) 0.004(3) -0.002(3) C2 0.006(3) 0.005(3) 0.010(3) -0.001(2) 0.003(3) 0.001(3) C3 0.005(3) 0.011(3) 0.012(3) -0.002(2) -0.003(2) -0.001(2) C4 0.010(3) 0.010(3) 0.015(3) -0.002(3) 0.003(3) -0.002(3) C5 0.010(4) 0.003(3) 0.015(4) 0.003(2) 0.003(3) 0.000(3) C6 0.007(4) 0.006(3) 0.024(4) 0.000(3) 0.002(3) -0.003(3) C7 0.015(4) 0.012(3) 0.014(4) -0.001(3) 0.005(3) 0.006(3) C8 0.003(3) 0.013(3) 0.009(3) 0.002(2) -0.002(2) 0.000(2) O1 0.015(3) 0.008(2) 0.024(3) 0.0015(19) 0.013(2) 0.004(2) O2 0.016(3) 0.011(2) 0.014(3) -0.0020(18) 0.005(2) 0.005(2) O3 0.005(2) 0.024(3) 0.024(3) 0.001(2) 0.004(2) -0.004(2) O4 0.010(3) 0.034(3) 0.022(3) -0.011(2) 0.006(2) -0.001(2) O5 0.016(3) 0.017(3) 0.010(3) -0.0016(19) 0.008(2) -0.007(2) O6 0.013(2) 0.010(2) 0.008(2) -0.0066(17) 0.0044(19) 0.0008(18) O7 0.010(3) 0.013(2) 0.022(3) -0.003(2) -0.001(2) 0.004(2) O8 0.013(3) 0.013(2) 0.014(3) -0.0020(19) 0.006(2) 0.001(2) Pb1 0.00678(15) 0.01051(15) 0.01076(15) 0.00031(10) 0.00223(9) 0.00055(12) S1 0.0073(8) 0.0098(7) 0.0102(8) -0.0003(6) 0.0010(7) -0.0001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.240(7) . ? C1 O1 1.269(7) . ? C1 C2 1.511(9) . ? C2 C3 1.385(9) . ? C2 C8 1.424(8) . ? C3 C4 1.388(9) . ? C3 H3 0.9500 . ? C4 C5 1.382(9) . ? C4 H4 0.9500 . ? C5 C7 1.383(9) . ? C5 C6 1.501(9) . ? C6 O3 1.214(8) . ? C6 O4 1.319(8) . ? C7 C8 1.389(9) . ? C7 H7 0.9500 . ? C8 S1 1.761(7) . ? O1 Pb1 2.520(4) 3_657 ? O1 Pb1 2.557(4) . ? O2 Pb1 2.656(4) 1_565 ? O3 Pb1 2.606(5) 3_757 ? O4 H4A 0.8400 . ? O5 S1 1.463(4) . ? O5 Pb1 2.672(4) . ? O6 S1 1.461(4) . ? O6 Pb1 2.708(4) 4 ? O7 S1 1.457(5) . ? O8 H8A 0.841(19) . ? O8 H8B 0.849(19) . ? Pb1 O1 2.520(4) 3_657 ? Pb1 O3 2.606(5) 3_757 ? Pb1 O2 2.656(4) 1_545 ? Pb1 O6 2.708(4) 4_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 123.4(6) . . ? O2 C1 C2 120.0(5) . . ? O1 C1 C2 116.6(6) . . ? C3 C2 C8 119.3(6) . . ? C3 C2 C1 118.3(6) . . ? C8 C2 C1 122.3(6) . . ? C2 C3 C4 119.7(6) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 121.2(7) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C7 120.0(6) . . ? C4 C5 C6 118.1(6) . . ? C7 C5 C6 121.9(6) . . ? O3 C6 O4 124.6(7) . . ? O3 C6 C5 121.6(6) . . ? O4 C6 C5 113.9(6) . . ? C5 C7 C8 120.0(6) . . ? C5 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C2 119.8(6) . . ? C7 C8 S1 120.2(5) . . ? C2 C8 S1 120.0(5) . . ? C1 O1 Pb1 103.4(4) . 3_657 ? C1 O1 Pb1 144.5(4) . . ? Pb1 O1 Pb1 110.65(17) 3_657 . ? C1 O2 Pb1 146.2(4) . 1_565 ? C6 O3 Pb1 137.7(5) . 3_757 ? C6 O4 H4A 109.5 . . ? S1 O5 Pb1 145.1(3) . . ? S1 O6 Pb1 123.3(3) . 4 ? H8A O8 H8B 111(3) . . ? O1 Pb1 O1 69.35(17) 3_657 . ? O1 Pb1 O3 143.16(16) 3_657 3_757 ? O1 Pb1 O3 81.82(15) . 3_757 ? O1 Pb1 O2 116.19(15) 3_657 1_545 ? O1 Pb1 O2 160.11(15) . 1_545 ? O3 Pb1 O2 98.77(15) 3_757 1_545 ? O1 Pb1 O5 109.67(15) 3_657 . ? O1 Pb1 O5 67.66(14) . . ? O3 Pb1 O5 78.05(15) 3_757 . ? O2 Pb1 O5 92.90(13) 1_545 . ? O1 Pb1 O6 112.68(14) 3_657 4_556 ? O1 Pb1 O6 127.52(15) . 4_556 ? O3 Pb1 O6 67.56(14) 3_757 4_556 ? O2 Pb1 O6 69.66(14) 1_545 4_556 ? O5 Pb1 O6 137.63(14) . 4_556 ? O7 S1 O6 114.0(3) . . ? O7 S1 O5 113.2(3) . . ? O6 S1 O5 111.1(3) . . ? O7 S1 C8 105.1(3) . . ? O6 S1 C8 106.6(3) . . ? O5 S1 C8 106.2(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.327 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.251 # Attachment '4448_web_deposit_cif_file_4_YixiaRen_1298976645.cif' data_110111a_0m _database_code_depnum_ccdc_archive 'CCDC 815047' #TrackingRef '4448_web_deposit_cif_file_4_YixiaRen_1298976645.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 N2 O15 Pb3 S2' _chemical_formula_weight 1282.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9683(12) _cell_length_b 7.5316(12) _cell_length_c 30.887(5) _cell_angle_alpha 85.113(3) _cell_angle_beta 84.509(3) _cell_angle_gamma 63.010(2) _cell_volume 1436.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1440 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 24.20 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 17.769 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0699 _exptl_absorpt_correction_T_max 0.4703 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7283 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0890 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5134 _reflns_number_gt 4085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5134 _refine_ls_number_parameters 433 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1341 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.307(2) 0.3814(19) 0.2883(5) 0.019(3) Uani 1 1 d . . . C2 C 0.527(2) 0.3308(19) 0.2805(5) 0.020(3) Uani 1 1 d U . . C3 C 0.641(2) 0.330(2) 0.2377(4) 0.015(3) Uani 1 1 d U . . C4 C 0.652(2) 0.2800(19) 0.3179(5) 0.021(3) Uani 1 1 d . . . H4 H 0.7963 0.2542 0.3142 0.026 Uiso 1 1 calc R . . C5 C 0.563(2) 0.269(2) 0.3586(5) 0.027(4) Uani 1 1 d . . . H5 H 0.6475 0.2365 0.3824 0.032 Uiso 1 1 calc R . . C6 C 0.351(2) 0.304(2) 0.3653(5) 0.023(3) Uani 1 1 d U . . C7 C 0.261(3) 0.281(2) 0.4088(6) 0.036(4) Uani 1 1 d . . . C8 C 0.221(2) 0.365(2) 0.3293(4) 0.022(3) Uani 1 1 d . . . H8 H 0.0757 0.3932 0.3335 0.027 Uiso 1 1 calc R . . C9 C 0.237(3) 0.898(2) 0.2991(6) 0.040(4) Uani 1 1 d . . . H9 H 0.1405 0.9435 0.2772 0.048 Uiso 1 1 calc R . . C10 C 0.161(2) 0.877(2) 0.3426(6) 0.036(4) Uani 1 1 d . . . H10 H 0.0175 0.9045 0.3491 0.043 Uiso 1 1 calc R . . C11 C 0.305(2) 0.815(2) 0.3757(5) 0.023(3) Uani 1 1 d . . . C12 C 0.514(3) 0.774(3) 0.3636(5) 0.042(4) Uani 1 1 d . . . H12 H 0.6165 0.7284 0.3844 0.050 Uiso 1 1 calc R . . C13 C 0.571(3) 0.799(3) 0.3210(5) 0.042(4) Uani 1 1 d . . . H13 H 0.7136 0.7746 0.3140 0.050 Uiso 1 1 calc R . . C14 C 0.228(3) 0.790(2) 0.4228(5) 0.035(4) Uani 1 1 d . . . C15 C 0.041(3) 0.772(3) 0.4330(6) 0.049(5) Uani 1 1 d . . . H15 H -0.0433 0.7783 0.4108 0.059 Uiso 1 1 calc R . . C16 C -0.021(3) 0.745(3) 0.4750(7) 0.054(5) Uani 1 1 d U . . H16 H -0.1501 0.7369 0.4807 0.065 Uiso 1 1 calc R . . C17 C 0.276(3) 0.746(3) 0.4986(6) 0.050(5) Uani 1 1 d . . . H17 H 0.3592 0.7378 0.5211 0.060 Uiso 1 1 calc R . . C18 C 0.347(3) 0.774(3) 0.4573(6) 0.051(5) Uani 1 1 d . . . H18 H 0.4771 0.7816 0.4523 0.061 Uiso 1 1 calc R . . C19 C 0.821(2) 0.6558(18) 0.1048(5) 0.017(3) Uani 1 1 d . . . C20 C 0.779(2) 0.783(2) 0.0642(5) 0.019(3) Uani 1 1 d U . . C21 C 0.7129(19) 0.9927(17) 0.0643(4) 0.012(3) Uani 1 1 d U . . C22 C 0.697(2) 1.1060(18) 0.0261(4) 0.014(3) Uani 1 1 d U . . H22 H 0.6573 1.2414 0.0269 0.017 Uiso 1 1 calc R . . C23 C 0.741(2) 1.0190(19) -0.0132(5) 0.018(3) Uani 1 1 d . . . C24 C 0.725(2) 1.140(2) -0.0543(5) 0.021(3) Uani 1 1 d . . . C25 C 0.796(2) 0.813(2) -0.0145(5) 0.022(3) Uani 1 1 d U . . H25 H 0.8235 0.7529 -0.0410 0.026 Uiso 1 1 calc R . . C26 C 0.810(2) 0.7045(19) 0.0238(5) 0.026(4) Uani 1 1 d . . . H26 H 0.8408 0.5711 0.0227 0.032 Uiso 1 1 calc R . . N1 N 0.440(2) 0.8559(18) 0.2889(4) 0.030(3) Uani 1 1 d . . . N2 N 0.096(2) 0.729(2) 0.5090(5) 0.043(4) Uani 1 1 d . . . O1 O -0.0675(17) 0.4509(17) 0.2657(4) 0.043(3) Uani 1 1 d . . . O2 O 0.0974(19) 0.6427(17) 0.2278(5) 0.053(4) Uani 1 1 d . . . O3 O 0.2378(18) 0.3020(19) 0.2131(4) 0.050(3) Uani 1 1 d . . . O4 O 0.5814(16) 0.4896(14) 0.2131(3) 0.025(2) Uani 1 1 d . . . O5 O 0.7930(17) 0.1641(14) 0.2264(3) 0.032(3) Uani 1 1 d . . . O6 O 0.3659(19) 0.225(2) 0.4420(4) 0.054(4) Uani 1 1 d . . . O7 O 0.0525(18) 0.3211(18) 0.4119(4) 0.048(3) Uani 1 1 d . . . H7 H 0.0153 0.3054 0.4374 0.071 Uiso 1 1 calc R . . O8 O 0.6577(15) 0.6749(13) 0.1317(3) 0.023(2) Uani 1 1 d . . . O9 O 1.0061(15) 0.5300(14) 0.1103(4) 0.030(3) Uani 1 1 d . . . O10 O 0.8337(16) 0.9656(14) 0.1428(3) 0.027(2) Uani 1 1 d . . . O11 O 0.4545(18) 1.1309(17) 0.1323(4) 0.041(3) Uani 1 1 d . . . O12 O 0.6796(16) 1.2889(13) 0.1067(3) 0.026(2) Uani 1 1 d . . . O13 O 0.6470(19) 1.3256(15) -0.0536(4) 0.037(3) Uani 1 1 d . . . O14 O 0.7880(16) 1.0541(14) -0.0905(3) 0.029(2) Uani 1 1 d . . . O15 O 0.2681(14) -0.1156(12) 0.1881(3) 0.024(2) Uani 1 1 d . . . H15A H 0.1935 -0.1440 0.2143 0.029 Uiso 1 1 calc R . . Pb1 Pb 0.02976(8) 0.19398(7) 0.159411(19) 0.02143(17) Uani 1 1 d . . . Pb2 Pb 0.60542(8) 0.80943(8) 0.206334(19) 0.02429(17) Uani 1 1 d . . . Pb3 Pb 0.32802(8) 0.61507(8) 0.131957(18) 0.02075(17) Uani 1 1 d . . . S1 S 0.1298(6) 0.4495(6) 0.24549(12) 0.0246(8) Uani 1 1 d . . . S2 S 0.6647(5) 1.1033(5) 0.11506(11) 0.0179(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.019(7) 0.025(7) 0.015(8) -0.002(6) 0.002(6) -0.012(6) C2 0.028(6) 0.019(6) 0.017(7) 0.005(5) -0.004(5) -0.014(5) C3 0.016(6) 0.027(6) 0.009(6) -0.003(5) 0.003(5) -0.016(5) C4 0.017(7) 0.023(7) 0.021(9) 0.005(6) -0.010(6) -0.006(6) C5 0.022(7) 0.047(9) 0.020(9) 0.017(7) -0.007(6) -0.026(7) C6 0.028(6) 0.031(7) 0.011(7) 0.005(5) -0.010(5) -0.014(5) C7 0.047(10) 0.040(10) 0.030(11) -0.005(8) 0.000(8) -0.028(8) C8 0.026(8) 0.038(9) 0.005(8) -0.004(6) -0.001(6) -0.016(7) C9 0.038(10) 0.036(10) 0.031(11) 0.005(8) -0.010(8) -0.004(8) C10 0.021(8) 0.043(10) 0.036(11) -0.003(8) 0.004(7) -0.009(7) C11 0.030(8) 0.021(7) 0.014(8) -0.007(6) -0.007(6) -0.007(6) C12 0.043(10) 0.078(13) 0.014(10) 0.009(8) -0.006(8) -0.038(10) C13 0.051(11) 0.070(13) 0.012(9) -0.010(8) 0.002(8) -0.033(10) C14 0.044(10) 0.043(10) 0.023(10) -0.009(7) 0.007(8) -0.024(8) C15 0.044(11) 0.096(15) 0.023(11) 0.004(10) -0.006(8) -0.045(11) C16 0.053(6) 0.058(7) 0.058(7) 0.001(5) -0.001(5) -0.032(5) C17 0.047(11) 0.076(14) 0.020(11) 0.003(9) 0.006(8) -0.024(10) C18 0.046(11) 0.107(16) 0.022(11) -0.019(10) 0.001(8) -0.052(11) C19 0.011(7) 0.009(6) 0.026(9) -0.006(6) 0.003(6) 0.001(5) C20 0.018(6) 0.026(6) 0.014(6) 0.007(5) 0.004(5) -0.012(5) C21 0.013(4) 0.011(4) 0.007(4) 0.001(3) -0.004(3) -0.002(3) C22 0.016(6) 0.014(6) 0.006(6) -0.002(4) -0.003(5) -0.002(4) C23 0.019(7) 0.022(7) 0.012(8) 0.004(6) -0.003(6) -0.007(6) C24 0.015(7) 0.036(9) 0.012(8) 0.016(7) -0.007(6) -0.013(6) C25 0.022(6) 0.030(6) 0.009(6) -0.003(5) -0.001(5) -0.008(5) C26 0.019(7) 0.008(7) 0.042(11) 0.002(6) 0.008(7) 0.001(6) N1 0.035(8) 0.027(7) 0.020(8) 0.003(6) 0.005(6) -0.008(6) N2 0.054(10) 0.060(10) 0.015(8) 0.006(7) 0.006(7) -0.030(8) O1 0.032(6) 0.067(8) 0.041(8) 0.013(6) -0.009(5) -0.034(6) O2 0.044(7) 0.045(7) 0.078(11) 0.040(7) -0.030(7) -0.029(6) O3 0.041(7) 0.086(9) 0.027(8) -0.035(6) -0.001(5) -0.026(7) O4 0.041(6) 0.033(6) 0.010(6) 0.010(4) -0.009(4) -0.025(5) O5 0.044(7) 0.027(6) 0.017(6) 0.000(5) 0.007(5) -0.010(5) O6 0.047(7) 0.105(11) 0.014(7) 0.023(7) -0.011(6) -0.042(8) O7 0.041(7) 0.081(9) 0.028(8) 0.007(6) 0.002(6) -0.036(7) O8 0.023(5) 0.016(5) 0.024(6) 0.001(4) 0.001(4) -0.004(4) O9 0.026(6) 0.025(6) 0.039(7) 0.015(5) -0.010(5) -0.012(5) O10 0.044(6) 0.031(6) 0.010(6) 0.001(4) -0.007(5) -0.021(5) O11 0.042(7) 0.056(7) 0.037(8) -0.023(6) 0.013(5) -0.032(6) O12 0.037(6) 0.018(5) 0.028(7) -0.006(4) -0.002(5) -0.014(4) O13 0.057(8) 0.028(6) 0.022(7) 0.009(5) -0.007(6) -0.018(5) O14 0.035(6) 0.033(6) 0.013(6) 0.002(5) -0.008(5) -0.011(5) O15 0.024(5) 0.014(5) 0.028(6) 0.010(4) -0.007(5) -0.003(4) Pb1 0.0213(3) 0.0202(3) 0.0220(3) 0.0030(2) -0.0069(2) -0.0082(2) Pb2 0.0229(3) 0.0368(3) 0.0161(3) 0.0007(2) -0.0033(2) -0.0160(3) Pb3 0.0236(3) 0.0231(3) 0.0173(3) 0.0036(2) -0.0023(2) -0.0126(2) S1 0.0255(19) 0.045(2) 0.012(2) 0.0047(16) -0.0041(15) -0.0237(17) S2 0.0217(17) 0.0219(18) 0.0136(19) -0.0031(14) 0.0018(14) -0.0130(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C8 1.369(19) . ? C1 C2 1.405(19) . ? C1 S1 1.778(14) . ? C2 C4 1.430(18) . ? C2 C3 1.474(19) . ? C3 O5 1.267(16) . ? C3 O4 1.284(15) . ? C4 C5 1.36(2) . ? C4 H4 0.9300 . ? C5 C6 1.375(19) . ? C5 H5 0.9300 . ? C6 C8 1.414(18) . ? C6 C7 1.46(2) . ? C7 O6 1.244(19) . ? C7 O7 1.342(19) . ? C8 H8 0.9300 . ? C9 N1 1.32(2) . ? C9 C10 1.42(2) . ? C9 H9 0.9300 . ? C10 C11 1.40(2) . ? C10 H10 0.9300 . ? C11 C12 1.37(2) . ? C11 C14 1.53(2) . ? C12 C13 1.36(2) . ? C12 H12 0.9300 . ? C13 N1 1.321(19) . ? C13 H13 0.9300 . ? C14 C15 1.37(2) . ? C14 C18 1.38(2) . ? C15 C16 1.36(3) . ? C15 H15 0.9300 . ? C16 N2 1.35(2) . ? C16 H16 0.9300 . ? C17 N2 1.32(2) . ? C17 C18 1.36(2) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O9 1.221(15) . ? C19 O8 1.304(16) . ? C19 C20 1.480(18) . ? C20 C26 1.38(2) . ? C20 C21 1.430(17) . ? C21 C22 1.380(17) . ? C21 S2 1.769(13) . ? C22 C23 1.370(19) . ? C22 H22 0.9300 . ? C23 C25 1.422(18) . ? C23 C24 1.481(17) . ? C24 O13 1.248(17) . ? C24 O14 1.280(18) . ? C24 Pb3 2.844(13) 2_675 ? C25 C26 1.364(19) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? N1 Pb2 2.678(13) . ? O1 S1 1.451(11) . ? O2 S1 1.434(10) . ? O3 S1 1.445(12) . ? O3 Pb1 2.697(10) . ? O4 Pb2 2.480(9) . ? O5 Pb1 2.581(10) 1_655 ? O7 H7 0.8200 . ? O8 Pb2 2.526(10) . ? O8 Pb3 2.533(9) . ? O9 Pb3 2.749(9) 1_655 ? O10 S2 1.459(10) . ? O10 Pb1 2.740(9) 1_665 ? O11 S2 1.438(11) . ? O12 S2 1.448(9) . ? O12 Pb3 2.672(10) 1_565 ? O13 Pb3 2.427(11) 2_675 ? O14 Pb3 2.515(9) 2_675 ? O15 Pb2 2.271(9) 1_545 ? O15 Pb1 2.323(8) . ? O15 Pb3 2.643(10) 1_545 ? O15 H15A 0.9800 . ? Pb1 O5 2.581(10) 1_455 ? Pb1 O10 2.740(9) 1_445 ? Pb2 O15 2.271(9) 1_565 ? Pb3 O13 2.427(11) 2_675 ? Pb3 O14 2.515(9) 2_675 ? Pb3 O15 2.643(10) 1_565 ? Pb3 O12 2.672(10) 1_545 ? Pb3 O9 2.749(9) 1_455 ? Pb3 C24 2.844(13) 2_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 C1 C2 121.4(13) . . ? C8 C1 S1 116.1(10) . . ? C2 C1 S1 122.3(11) . . ? C1 C2 C4 116.8(13) . . ? C1 C2 C3 126.4(12) . . ? C4 C2 C3 116.8(12) . . ? O5 C3 O4 122.8(13) . . ? O5 C3 C2 116.6(11) . . ? O4 C3 C2 120.6(12) . . ? C5 C4 C2 121.1(13) . . ? C5 C4 H4 119.4 . . ? C2 C4 H4 119.4 . . ? C4 C5 C6 121.1(13) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C8 119.1(14) . . ? C5 C6 C7 120.5(13) . . ? C8 C6 C7 120.4(13) . . ? O6 C7 O7 119.5(16) . . ? O6 C7 C6 124.6(15) . . ? O7 C7 C6 115.9(14) . . ? C1 C8 C6 120.2(13) . . ? C1 C8 H8 119.9 . . ? C6 C8 H8 119.9 . . ? N1 C9 C10 121.7(15) . . ? N1 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C11 C10 C9 119.2(15) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C12 C11 C10 117.1(15) . . ? C12 C11 C14 122.5(13) . . ? C10 C11 C14 120.3(14) . . ? C13 C12 C11 119.4(15) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N1 C13 C12 125.2(17) . . ? N1 C13 H13 117.4 . . ? C12 C13 H13 117.4 . . ? C15 C14 C18 116.2(16) . . ? C15 C14 C11 121.8(15) . . ? C18 C14 C11 122.0(15) . . ? C16 C15 C14 120.7(17) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? N2 C16 C15 123.3(18) . . ? N2 C16 H16 118.3 . . ? C15 C16 H16 118.3 . . ? N2 C17 C18 124.6(18) . . ? N2 C17 H17 117.7 . . ? C18 C17 H17 117.7 . . ? C17 C18 C14 120.0(17) . . ? C17 C18 H18 120.0 . . ? C14 C18 H18 120.0 . . ? O9 C19 O8 123.2(13) . . ? O9 C19 C20 118.3(13) . . ? O8 C19 C20 118.4(11) . . ? C26 C20 C21 116.3(12) . . ? C26 C20 C19 121.8(12) . . ? C21 C20 C19 121.9(13) . . ? C22 C21 C20 121.4(12) . . ? C22 C21 S2 120.1(9) . . ? C20 C21 S2 118.4(9) . . ? C23 C22 C21 120.1(12) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C25 119.9(12) . . ? C22 C23 C24 120.1(12) . . ? C25 C23 C24 120.1(13) . . ? O13 C24 O14 120.2(12) . . ? O13 C24 C23 120.2(14) . . ? O14 C24 C23 119.5(13) . . ? O13 C24 Pb3 58.1(7) . 2_675 ? O14 C24 Pb3 62.2(7) . 2_675 ? C23 C24 Pb3 177.1(10) . 2_675 ? C26 C25 C23 118.9(13) . . ? C26 C25 H25 120.6 . . ? C23 C25 H25 120.6 . . ? C25 C26 C20 123.3(13) . . ? C25 C26 H26 118.3 . . ? C20 C26 H26 118.3 . . ? C9 N1 C13 117.4(15) . . ? C9 N1 Pb2 121.7(11) . . ? C13 N1 Pb2 119.7(11) . . ? C17 N2 C16 115.2(16) . . ? S1 O3 Pb1 123.8(6) . . ? C3 O4 Pb2 140.0(8) . . ? C3 O5 Pb1 113.6(8) . 1_655 ? C7 O7 H7 109.5 . . ? C19 O8 Pb2 122.0(8) . . ? C19 O8 Pb3 137.4(9) . . ? Pb2 O8 Pb3 100.6(3) . . ? C19 O9 Pb3 124.0(9) . 1_655 ? S2 O10 Pb1 101.4(4) . 1_665 ? S2 O12 Pb3 115.2(5) . 1_565 ? C24 O13 Pb3 96.0(9) . 2_675 ? C24 O14 Pb3 91.1(8) . 2_675 ? Pb2 O15 Pb1 123.9(4) 1_545 . ? Pb2 O15 Pb3 104.5(4) 1_545 1_545 ? Pb1 O15 Pb3 107.7(4) . 1_545 ? Pb2 O15 H15A 106.6 1_545 . ? Pb1 O15 H15A 106.6 . . ? Pb3 O15 H15A 106.6 1_545 . ? O15 Pb1 O5 80.8(3) . 1_455 ? O15 Pb1 O3 79.2(4) . . ? O5 Pb1 O3 88.0(4) 1_455 . ? O15 Pb1 O10 79.0(3) . 1_445 ? O5 Pb1 O10 69.1(3) 1_455 1_445 ? O3 Pb1 O10 150.5(4) . 1_445 ? O15 Pb2 O4 74.2(3) 1_565 . ? O15 Pb2 O8 75.0(3) 1_565 . ? O4 Pb2 O8 70.6(3) . . ? O15 Pb2 N1 86.3(4) 1_565 . ? O4 Pb2 N1 85.4(4) . . ? O8 Pb2 N1 152.7(4) . . ? O13 Pb3 O14 52.6(3) 2_675 2_675 ? O13 Pb3 O8 85.4(3) 2_675 . ? O14 Pb3 O8 77.5(3) 2_675 . ? O13 Pb3 O15 123.2(3) 2_675 1_565 ? O14 Pb3 O15 72.3(3) 2_675 1_565 ? O8 Pb3 O15 68.9(3) . 1_565 ? O13 Pb3 O12 77.4(3) 2_675 1_545 ? O14 Pb3 O12 122.1(3) 2_675 1_545 ? O8 Pb3 O12 70.4(3) . 1_545 ? O15 Pb3 O12 131.7(3) 1_565 1_545 ? O13 Pb3 O9 80.9(3) 2_675 1_455 ? O14 Pb3 O9 98.1(3) 2_675 1_455 ? O8 Pb3 O9 165.3(3) . 1_455 ? O15 Pb3 O9 123.6(3) 1_565 1_455 ? O12 Pb3 O9 101.1(3) 1_545 1_455 ? O13 Pb3 C24 25.9(4) 2_675 2_675 ? O14 Pb3 C24 26.7(4) 2_675 2_675 ? O8 Pb3 C24 80.2(3) . 2_675 ? O15 Pb3 C24 98.2(4) 1_565 2_675 ? O12 Pb3 C24 99.5(4) 1_545 2_675 ? O9 Pb3 C24 89.7(3) 1_455 2_675 ? O2 S1 O3 110.3(9) . . ? O2 S1 O1 112.3(7) . . ? O3 S1 O1 114.2(7) . . ? O2 S1 C1 107.9(7) . . ? O3 S1 C1 106.5(7) . . ? O1 S1 C1 105.2(7) . . ? O11 S2 O12 113.2(6) . . ? O11 S2 O10 111.7(7) . . ? O12 S2 O10 110.7(6) . . ? O11 S2 C21 107.0(6) . . ? O12 S2 C21 106.9(6) . . ? O10 S2 C21 107.1(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.689 _refine_diff_density_min -3.434 _refine_diff_density_rms 0.365 # Attachment '4449_web_deposit_cif_file_5_YixiaRen_1298976645.cif' data_101002b_0m _database_code_depnum_ccdc_archive 'CCDC 815048' #TrackingRef '4449_web_deposit_cif_file_5_YixiaRen_1298976645.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H4 O8 Pb2 S' _chemical_formula_weight 674.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.3119(8) _cell_length_b 22.365(3) _cell_length_c 7.5899(8) _cell_angle_alpha 90.00 _cell_angle_beta 111.923(2) _cell_angle_gamma 90.00 _cell_volume 1151.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 858 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 23.31 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 29.420 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0486 _exptl_absorpt_correction_T_max 0.3857 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6870 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2617 _reflns_number_gt 1954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00143(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2617 _refine_ls_number_parameters 173 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.797(2) 0.8246(5) 0.620(2) 0.042(4) Uani 1 1 d . . . C2 C 0.730(2) 0.7606(5) 0.5628(17) 0.034(3) Uani 1 1 d . . . C3 C 0.8630(19) 0.7150(5) 0.6505(16) 0.028(3) Uani 1 1 d . . . H3 H 0.9861 0.7238 0.7420 0.034 Uiso 1 1 calc R . . C4 C 0.8090(19) 0.6570(5) 0.5995(16) 0.027(3) Uani 1 1 d . . . C5 C 0.6251(17) 0.6424(4) 0.4589(16) 0.023(2) Uani 1 1 d U . . C6 C 0.5616(18) 0.5805(4) 0.3844(16) 0.022(2) Uani 1 1 d . . . C7 C 0.492(2) 0.6883(5) 0.3790(19) 0.034(3) Uani 1 1 d . . . H7 H 0.3659 0.6792 0.2935 0.041 Uiso 1 1 calc R . . C8 C 0.543(2) 0.7477(5) 0.4247(17) 0.032(3) Uani 1 1 d . . . H8 H 0.4563 0.7784 0.3650 0.038 Uiso 1 1 calc R . . O1 O 0.9606(16) 0.8313(4) 0.7490(14) 0.048(3) Uani 1 1 d . . . O2 O 0.6916(15) 0.8673(3) 0.5379(12) 0.042(2) Uani 1 1 d . . . O3 O 1.1236(17) 0.6295(4) 0.8922(14) 0.058(3) Uani 1 1 d . . . O4 O 1.0681(13) 0.5745(4) 0.6049(13) 0.037(2) Uani 1 1 d . . . O5 O 0.8644(16) 0.5556(4) 0.7834(15) 0.048(3) Uani 1 1 d . . . O6 O 0.6821(14) 0.5481(3) 0.3428(12) 0.036(2) Uani 1 1 d . . . O7 O 0.3951(14) 0.5626(4) 0.3689(14) 0.042(2) Uani 1 1 d . . . O8 O 0.6922(12) 1.0097(3) 0.5233(12) 0.0293(19) Uani 1 1 d . . . H8A H 0.7479 1.0415 0.4697 0.035 Uiso 1 1 calc R . . Pb1 Pb 0.52770(7) 1.04926(2) 0.71323(7) 0.02977(17) Uani 1 1 d . . . Pb2 Pb 0.96267(7) 0.939440(19) 0.73867(7) 0.03077(17) Uani 1 1 d . . . S1 S 0.9780(5) 0.60090(12) 0.7303(5) 0.0303(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.053(10) 0.030(6) 0.039(8) 0.004(5) 0.012(8) 0.009(7) C2 0.043(9) 0.030(6) 0.025(7) 0.003(5) 0.009(6) 0.004(6) C3 0.028(7) 0.031(5) 0.022(6) 0.001(5) 0.005(5) -0.008(5) C4 0.030(7) 0.033(6) 0.023(7) 0.006(5) 0.015(6) 0.004(5) C5 0.015(5) 0.020(4) 0.034(6) -0.003(4) 0.009(5) -0.001(4) C6 0.024(6) 0.024(5) 0.019(6) -0.006(4) 0.007(5) -0.005(5) C7 0.025(7) 0.030(6) 0.041(8) -0.001(5) 0.004(6) -0.007(5) C8 0.038(8) 0.025(5) 0.028(7) -0.008(5) 0.006(6) 0.006(5) O1 0.044(7) 0.029(5) 0.057(7) -0.008(4) 0.002(5) 0.000(4) O2 0.054(7) 0.027(4) 0.035(5) 0.004(3) 0.006(5) 0.012(4) O3 0.060(8) 0.036(5) 0.048(6) -0.007(4) -0.014(6) 0.015(5) O4 0.022(5) 0.046(5) 0.045(6) 0.008(4) 0.015(4) 0.013(4) O5 0.052(7) 0.041(5) 0.059(7) 0.016(4) 0.031(6) 0.004(5) O6 0.038(6) 0.035(4) 0.030(5) -0.008(4) 0.005(4) -0.005(4) O7 0.025(5) 0.043(5) 0.061(7) -0.004(4) 0.021(5) -0.006(4) O8 0.026(5) 0.026(4) 0.037(5) 0.000(3) 0.014(4) 0.000(3) Pb1 0.0274(3) 0.0311(2) 0.0280(3) -0.00292(16) 0.0070(2) 0.00324(19) Pb2 0.0257(3) 0.0275(2) 0.0379(3) 0.00058(17) 0.0104(2) -0.00053(19) S1 0.0305(18) 0.0239(13) 0.0338(18) 0.0003(11) 0.0086(15) 0.0052(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.238(15) . ? C1 O1 1.242(16) . ? C1 C2 1.522(17) . ? C1 Pb2 2.840(13) . ? C2 C3 1.396(16) . ? C2 C8 1.404(17) . ? C3 C4 1.368(15) . ? C3 H3 0.9300 . ? C4 C5 1.408(16) . ? C4 S1 1.781(12) . ? C5 C7 1.390(16) . ? C5 C6 1.502(14) . ? C6 O7 1.245(15) . ? C6 O6 1.269(14) . ? C7 C8 1.389(15) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? O1 Pb2 2.419(9) . ? O2 Pb2 2.569(9) . ? O2 Pb1 2.722(8) 3_676 ? O3 S1 1.441(9) . ? O4 S1 1.468(9) . ? O4 Pb2 2.611(9) 4_575 ? O5 S1 1.459(10) . ? O6 Pb2 2.474(10) 4_575 ? O6 Pb1 2.480(8) 4_575 ? O8 Pb1 2.322(8) 3_676 ? O8 Pb1 2.367(8) . ? O8 Pb2 2.576(8) . ? O8 H8A 0.9800 . ? Pb1 O8 2.322(8) 3_676 ? Pb1 O6 2.480(8) 4_576 ? Pb1 O2 2.722(8) 3_676 ? Pb2 O6 2.474(10) 4_576 ? Pb2 O4 2.611(9) 4_576 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 122.5(13) . . ? O2 C1 C2 120.6(13) . . ? O1 C1 C2 116.9(11) . . ? O2 C1 Pb2 64.7(7) . . ? O1 C1 Pb2 57.8(7) . . ? C2 C1 Pb2 173.9(11) . . ? C3 C2 C8 121.1(11) . . ? C3 C2 C1 117.3(12) . . ? C8 C2 C1 121.6(11) . . ? C4 C3 C2 118.8(12) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 121.8(11) . . ? C3 C4 S1 116.3(10) . . ? C5 C4 S1 121.8(8) . . ? C7 C5 C4 118.4(10) . . ? C7 C5 C6 116.7(10) . . ? C4 C5 C6 124.9(10) . . ? O7 C6 O6 122.6(10) . . ? O7 C6 C5 119.1(11) . . ? O6 C6 C5 118.3(11) . . ? C8 C7 C5 121.1(12) . . ? C8 C7 H7 119.4 . . ? C5 C7 H7 119.4 . . ? C7 C8 C2 118.7(11) . . ? C7 C8 H8 120.7 . . ? C2 C8 H8 120.7 . . ? C1 O1 Pb2 96.4(8) . . ? C1 O2 Pb2 89.4(8) . . ? C1 O2 Pb1 167.0(9) . 3_676 ? Pb2 O2 Pb1 96.1(3) . 3_676 ? S1 O4 Pb2 135.4(5) . 4_575 ? C6 O6 Pb2 138.7(7) . 4_575 ? C6 O6 Pb1 110.2(7) . 4_575 ? Pb2 O6 Pb1 106.3(3) 4_575 4_575 ? Pb1 O8 Pb1 108.7(3) 3_676 . ? Pb1 O8 Pb2 106.9(3) 3_676 . ? Pb1 O8 Pb2 106.6(3) . . ? Pb1 O8 H8A 111.5 3_676 . ? Pb1 O8 H8A 111.5 . . ? Pb2 O8 H8A 111.5 . . ? O8 Pb1 O8 71.3(3) 3_676 . ? O8 Pb1 O6 83.7(3) 3_676 4_576 ? O8 Pb1 O6 69.7(3) . 4_576 ? O8 Pb1 O2 77.9(3) 3_676 3_676 ? O8 Pb1 O2 97.5(3) . 3_676 ? O6 Pb1 O2 160.3(3) 4_576 3_676 ? O1 Pb2 O6 95.0(3) . 4_576 ? O1 Pb2 O2 51.6(3) . . ? O6 Pb2 O2 73.3(3) 4_576 . ? O1 Pb2 O8 128.1(3) . . ? O6 Pb2 O8 66.6(3) 4_576 . ? O2 Pb2 O8 76.5(3) . . ? O1 Pb2 O4 81.3(3) . 4_576 ? O6 Pb2 O4 67.9(3) 4_576 4_576 ? O2 Pb2 O4 114.3(3) . 4_576 ? O8 Pb2 O4 126.8(3) . 4_576 ? O1 Pb2 C1 25.7(3) . . ? O6 Pb2 C1 84.0(4) 4_576 . ? O2 Pb2 C1 25.8(3) . . ? O8 Pb2 C1 102.4(4) . . ? O4 Pb2 C1 98.7(3) 4_576 . ? O3 S1 O5 112.8(7) . . ? O3 S1 O4 111.3(7) . . ? O5 S1 O4 109.8(6) . . ? O3 S1 C4 107.5(5) . . ? O5 S1 C4 107.1(6) . . ? O4 S1 C4 108.0(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.768 _refine_diff_density_min -1.840 _refine_diff_density_rms 0.338